CN113466221B - High polymer material thermal vacuum stability testing device and testing method - Google Patents
High polymer material thermal vacuum stability testing device and testing method Download PDFInfo
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- CN113466221B CN113466221B CN202110697694.9A CN202110697694A CN113466221B CN 113466221 B CN113466221 B CN 113466221B CN 202110697694 A CN202110697694 A CN 202110697694A CN 113466221 B CN113466221 B CN 113466221B
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Abstract
The invention belongs to the field of chemical detection, and particularly relates to a device and a method for testing thermal vacuum stability of a high polymer material. The test device includes: heating pipe, heating pipe evacuating device, heater. The heating pipe is internally provided with a volatile organic compound inspection part, the surface of the volatile organic compound inspection part is a plating layer or a coating containing at least one element of silver, iron, nickel or copper, or the whole volatile organic compound inspection part is a part containing at least one element of silver, iron, nickel or copper. In the testing device and the testing method, if organic matters are precipitated, the organic matters and the volatile organic matter inspection part are subjected to chemical reaction to generate color change, and the color change can be identified by naked eyes. Therefore, the testing device and the testing method can qualitatively display the precipitation of the organic small molecular volatile matters in the high molecular material, namely, the thermal vacuum stability of the high molecular material is detected.
Description
Technical Field
The invention belongs to the field of chemical detection, and particularly relates to a device and a method for testing thermal vacuum stability of a high polymer material.
Background
The organic small molecules are mostly contained in polymer composite materials, organic matters and the like, and are more easily separated out, adsorbed and deposited on the surfaces of various precision devices under the conditions of high temperature and vacuum. Under specific conditions, the corrosion oxidation effect on metal base and the like can be generated. The detection of the corrosion of organic micromolecular metal under high-temperature vacuum is one of important evaluation indexes for the stability of polymer composite materials and organic matters.
The method for testing the corrosion of the organic micromolecule metal under high-temperature vacuum at home and abroad is still a blank. Only some of these provide the testing criteria for volatile organics, such as: QJ 1558B-2016 Standard: after a certain temperature (140 ℃), the volatile organic compounds condense on the metal surface, and the volatile organic compound percentage is obtained after weighing.
However, the above method has the following problems:
1. colorless volatile organic compounds are almost difficult to identify by naked eyes, and a method with a display effect for qualitatively representing the volatilization of small molecules is lacked. 2. The organic small molecules can not be continuously and systematically observed to be separated out. 3. At present, a qualitative and quantitative detection method is not available.
The present invention has been made to solve the above problems.
Disclosure of Invention
The invention provides a high polymer material thermal vacuum stability testing device in a first aspect, which comprises: the heating device comprises a heating pipe, a heating pipe vacuumizing device and a heater;
the heating pipe vacuumizing device is used for vacuumizing the heating pipe;
the heater is used for heating the heating pipe;
the heating pipe is internally provided with a volatile organic compound inspection part, the surface of the volatile organic compound inspection part is a plating layer or a coating containing at least one element of silver, iron, nickel or copper, or the whole volatile organic compound inspection part is a part containing at least one element of silver, iron, nickel or copper.
Preferably, the heating tube is a quartz tube.
Preferably, the heater is a high temperature oven or a muffle furnace, and is set at room temperature to 1100 ℃.
Preferably, the volatile organic compound inspection part is a silver-plated sheet, a copper, iron, nickel or zinc sheet.
Preferably, the test apparatus further comprises: a controller;
the controller is in communication connection with the heating pipe vacuumizing device and/or the heater and is used for controlling the operation program of the heating cavity vacuumizing device and/or controlling the heating program of the heater.
The second aspect of the present invention provides a method for testing thermal vacuum stability of a polymer material, wherein the method comprises the following steps:
step 1, putting a high polymer material to be tested into a heating pipe, sealing the heating pipe, starting a heating pipe vacuumizing device to vacuumize the heating pipe, starting a heater to heat the heating pipe, and analyzing the stability of the high polymer material to be tested according to the color change of the volatile organic compound inspection part after a period of time;
the analysis method comprises the following steps:
compared with the initial state of the volatile organic compound inspection part, if the volatile organic compound inspection part has color change, the high polymer material to be tested is unstable at the temperature;
compared with the initial state of the volatile organic compound inspection part, if the volatile organic compound inspection part does not have color change, the high polymer material to be tested is stable at the temperature.
Preferably, if the region with color change and the color depth of the volatile organic compound inspection part do not change any more after the heating time is prolonged compared with the initial state of the volatile organic compound inspection part, it indicates that the volatile organic compound of the polymer material to be tested has been completely precipitated.
Preferably, the test method can also quantitatively determine the quality of the volatile organic compounds, and comprises the following specific steps:
measuring the area of the region with the color change of the volatile organic compound inspection part and the mass loss of the same type of high polymer material to be tested for many times, and then establishing a correlation formula between the area A of the region with the color change of the volatile organic compound inspection part and the mass loss M of the same type of high polymer material to be tested;
and finally, substituting the area of the region with the color change of the volatile organic compound inspection part in a certain determination process into a correlation formula to calculate the mass loss of the high polymer material to be tested.
Preferably, the vacuum degree in the heating tube is that the absolute pressure value is 10 -6 ～10 -4 Pa。
Preferably, the heating temperature of the heating pipe is 100-900 ℃, and the heating time is 1-24 hours.
The polymer material to be tested comprises: polymeric materials that volatilize small organic molecules at high temperatures.
Compared with the prior art, the invention has the following beneficial effects:
1. the prior art can not observe the organic micromolecule separation of the high molecular material continuously and systematically. In the testing device and the testing method, if organic matters are precipitated, the organic matters and the volatile organic matter inspection part are subjected to chemical reaction to generate color change, and the color change can be identified by naked eyes. Therefore, the testing device and the testing method can qualitatively display the precipitation of the organic small molecular volatile matters in the high molecular material, namely, the thermal vacuum stability of the high molecular material is detected.
In addition, the method can quantitatively calculate the mass of the organic small molecule volatile according to the area of the region with the color change of the volatile organic compound inspection part and a correlation formula between the area A of the region with the color change of the volatile organic compound inspection part and the mass loss M of the same type of high molecular material to be detected.
2. The device has controllable vacuum degree and adjustable temperature gradient, and can be used for measuring the separation of organic micromolecular volatile matters in the high polymer material under various vacuum degrees and various temperatures, namely detecting the thermal vacuum stability of the high polymer material.
3. The prior art measurement method cannot show the termination of the organic small-molecule volatile matter precipitation in the high molecular material, so that whether the organic small-molecule volatile matter precipitation is terminated or not can be proved only by measuring for a plurality of times in a prolonged time. The invention can judge whether the separation of the organic micromolecule volatile matter is stopped or not only according to the color change of the volatile organic matter checking component.
4. The measuring method of the invention is suitable for measuring various organic small molecule volatile matters precipitated in high molecular materials, and does not require the condensation of the organic small molecule volatile matters on the surface of a device, so the measuring method is not limited to volatile organic matters.
In conclusion, the determination method of the invention is more flexible, convenient and accurate.
Drawings
FIG. 1 is a graph showing the effect of example 2 after tube sealing and vacuum calcination.
FIG. 2 is a graph showing the effects of comparative example 1 after calcination.
Detailed Description
The present invention is further illustrated by the following examples, but is not limited to these examples. The experimental methods not specified in the examples are generally commercially available according to the conventional conditions and the conditions described in the manual, or according to the general-purpose equipment, materials, reagents and the like used under the conditions recommended by the manufacturer, unless otherwise specified. The starting materials required in the following examples and comparative examples are all commercially available.
Example 1
A high polymer material thermal vacuum stability testing device, the testing device comprises: high-purity quartz tube, evacuating device, heater.
The heating pipe vacuumizing device comprises a mechanical pump and a molecular pump.
The heater is used for heating the heating pipe, and the heater is specifically a muffle furnace.
A volatile organic compound inspection part is arranged in the high-purity quartz tube and is an aluminum alloy silver-plated sheet.
The controller is in communication connection with the heating pipe vacuumizing device and is used for controlling the operation program of the heating cavity vacuumizing device.
Example 2
A method for testing thermal vacuum stability of a high polymer material comprises the following steps:
the polymer material to be detected is a polymer sheet, specifically a patch compounded by polyphenylene sulfide, epoxy resin and the like with inorganic materials.
Fixing the high polymer material sheet to be detected and the aluminum alloy silver-plated sheet, sealing the fixed high polymer material sheet and the aluminum alloy silver-plated sheet together in a high-purity quartz tube, pumping for 10 minutes by using a mechanical pump, and pumping for 10 minutes by using a molecular pump to ensure that the vacuum degree in the quartz tube is 10 -6 ～10 -4 Pa (high vacuum degree), and sealing the quartz tube.
Then, the quartz tube was placed in a muffle furnace, and the quartz tube was heated according to the following heating procedure:
initially, marking the aluminum alloy silver-plated sheet as a sample 0, heating to 100 ℃, and keeping for 12 hours to obtain a sample 1; then, continuously heating the sample 1 to 180 ℃, and keeping for 5 hours to obtain a sample 2; then, continuously heating the sample 2 to 200 ℃, and keeping for 2 hours to obtain a sample 3; sample 3 was then heated to 220 degrees celsius for 2 hours to yield sample 4.
The results are as follows:
as shown in fig. 1, from left to right: sample 0, sample 1, sample 2, sample 3, sample 4.
The silvery white of sample 1 did not change significantly compared to sample 0, indicating that no oxidation of Ag occurred at high vacuum. Compared with sample 1, brown precipitates appear on the surface of sample 2, namely volatile organic matters in the to-be-detected high polymer material are precipitated and directly undergo redox reaction with Ag to generate silver oxide. Sample 3 was not significantly changed compared to sample 2; sample 4 also did not change significantly, i.e. the volatile organics were considered to have evolved.
Other metals, such as iron and volatile organic compounds, can also generate colored ferroferric oxide and/or ferric oxide after reacting at high temperature, copper and volatile organic compounds can also generate colored cuprous oxide and/or copper oxide after reacting at high temperature, finally, precipitates of various colors are shown on the surface of the sample, the color of the precipitates is greatly different from that of the original metal, and the precipitates can be identified by naked eyes. Therefore, experimental confirmation is not necessarily arranged.
Comparative example 1
The silver-plated aluminum alloy test piece in example 1 was directly calcined in air at 180 ℃ for 5 hours. The aluminum alloy silver-plated test piece after calcination is shown in fig. 2 as control sample 1.
The result is shown in fig. 2, from left to right: sample 0, comparative sample 1.
After the aluminum alloy silver-plated test piece is calcined, brown precipitates appear on the surface, namely, oxygen and Ag undergo redox reaction to generate silver oxide.
This proves that the brown precipitate in example 1 is actually silver oxide formed by the reaction of the oxygen-containing molecule with Ag. Indirectly proves that volatile organic compounds are separated out from the high polymer material to be detected. The volatile organic compounds are small molecular organic compounds.
Comparative example 2
The aluminum alloy silver-plated test piece in example 1 was directly calcined in the apparatus of example 1. The only differences from example 1 are: there is no polymer material to be tested. After the quartz tube is heated according to the same heating procedure, the appearance of the aluminum alloy silver-plated test piece is not changed all the time. The result proves that the appearance change of the aluminum alloy silver-plated test piece is really the result of the precipitation of the volatile organic compounds of the high polymer material to be tested.
Claims (1)
1. A method for testing thermal vacuum stability of a polymer material is characterized by using the following polymer material thermal vacuum stability testing device, wherein the testing device comprises: the heating device comprises a heating pipe, a heating pipe vacuumizing device and a heater;
the heating pipe vacuumizing device is used for vacuumizing the heating pipe;
the heater is used for heating the heating pipe;
a volatile organic compound inspection part is arranged in the heating pipe,
the volatile organic compound inspection part is a silver-plated sheet, a copper-plated sheet, an iron-plated sheet, a nickel-plated sheet or a zinc-plated sheet;
the test method comprises the following steps:
step 1, putting a high polymer material to be tested into a heating pipe, sealing the heating pipe, starting a heating pipe vacuumizing device to vacuumize the heating pipe, starting a heater to heat the heating pipe, and analyzing the stability of the high polymer material to be tested according to the color change of the volatile organic compound inspection part after a period of time;
the analysis method comprises the following steps: compared with the initial state of the volatile organic compound inspection part, if the color of the volatile organic compound inspection part changes, the high polymer material to be tested is unstable at the temperature; compared with the initial state of the volatile organic compound inspection part, if the volatile organic compound inspection part does not have color change, the high polymer material to be tested is stable at the temperature;
if the heating time is prolonged, compared with the initial state of the volatile organic compound inspection part, if the region with color change and the color depth of the volatile organic compound inspection part are not changed, the volatile organic compound of the high polymer material to be tested is completely separated out;
the test method can also be used for quantitatively measuring the quality of the volatile organic compounds, and comprises the following specific steps:
measuring the area of the region with the color change of the volatile organic compound inspection part and the mass loss of the same type of high polymer material to be tested for many times, and then establishing a correlation formula between the area A of the region with the color change of the volatile organic compound inspection part and the mass loss M of the same type of high polymer material to be tested;
finally, substituting the area of the region with color change of the volatile organic compound inspection part in a certain determination process into a correlation formula to calculate the mass loss of the high polymer material to be tested;
the vacuum degree in the heating tube is that the absolute pressure value is 10 -6 ～10 -4 Pa；
The heating temperature of the heating pipe is 100-900 ℃, and the heating time is 1-24 hours.
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| EP0247789A3 (en) * | 1986-05-27 | 1989-08-02 | The BOC Group, Inc. | Gas constituent measurement and recording |
| US4927766A (en) * | 1986-05-27 | 1990-05-22 | The Boc Group, Inc. | Gas constituent measurement and recording |
| WO1990003999A1 (en) * | 1988-10-07 | 1990-04-19 | M&T Chemicals Inc. | Improved stabilizers for halogen-containing polymers |
| US5320807A (en) * | 1993-05-07 | 1994-06-14 | Brinton William F | Test kits for determining the chemical stability of a compost sample |
| US5445795A (en) * | 1993-11-17 | 1995-08-29 | The United States Of America As Represented By The United States Department Of Energy | Volatile organic compound sensing devices |
| JP2002243718A (en) * | 2001-02-19 | 2002-08-28 | Sony Corp | Detection tool for suspended toxic substance, its manufacturing method, and method for detection using the same |
| EP2040071A3 (en) * | 2007-09-18 | 2014-01-01 | HY-Energy LLP | Gas sorption tester for rapid screening of multiple samples |
| CN101747380A (en) * | 2008-12-08 | 2010-06-23 | 中国科学院福建物质结构研究所 | Pyridine alkyne complex gas sensitive material of metal platinum |
| CN101832983A (en) * | 2010-05-19 | 2010-09-15 | 南昌大学 | Method for measuring volatile substance release in interior wall coating |
| US9376435B2 (en) * | 2011-09-23 | 2016-06-28 | Jawaharlal Nehru Centre For Advanced Scientific Research | Chromophores for the detection of volatile organic compounds |
| CN104237057A (en) * | 2014-09-05 | 2014-12-24 | 兰州空间技术物理研究所 | Characteristic testing method of condensable and volatile matters in non-metal material in vacuum |
| TWI627403B (en) * | 2015-10-08 | 2018-06-21 | 五鼎生物技術股份有限公司 | Biochemical test chip |
| CN107037070B (en) * | 2016-02-04 | 2023-08-11 | 固安鼎材科技有限公司 | Method for detecting thermal stability of small molecular material, testing device and system |
| WO2018070360A1 (en) * | 2016-10-11 | 2018-04-19 | 株式会社村田製作所 | Volatile organic substance detection body and manufacturing method therefor, volatile organic substance detection method, and volatile organic substance detection device |
| KR102036969B1 (en) * | 2017-10-25 | 2019-10-25 | 한국과학기술원 | Composite nanofiber membrane colorimetric gas sensors including hydrophillic cellulose fibrils comprising metal organic framework particles and color change dye and manufacturing method thereof |
| CN110987822B (en) * | 2019-11-19 | 2022-07-05 | 广西大学 | Method for detecting volatile organic compound |
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